CN117210100A - Powder coating and preparation method and application thereof - Google Patents
Powder coating and preparation method and application thereof Download PDFInfo
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- CN117210100A CN117210100A CN202311420782.XA CN202311420782A CN117210100A CN 117210100 A CN117210100 A CN 117210100A CN 202311420782 A CN202311420782 A CN 202311420782A CN 117210100 A CN117210100 A CN 117210100A
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- 239000011248 coating agent Substances 0.000 title claims abstract description 141
- 239000000843 powder Substances 0.000 title claims abstract description 137
- 238000002360 preparation method Methods 0.000 title abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 80
- 229920001971 elastomer Polymers 0.000 claims abstract description 71
- 239000002131 composite material Substances 0.000 claims abstract description 52
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 229920005989 resin Polymers 0.000 claims abstract description 29
- 239000011347 resin Substances 0.000 claims abstract description 29
- 239000012970 tertiary amine catalyst Substances 0.000 claims abstract description 29
- 239000002253 acid Substances 0.000 claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 10
- 239000000945 filler Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 4
- 238000001723 curing Methods 0.000 claims description 97
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- 238000000034 method Methods 0.000 claims description 25
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- 229920001225 polyester resin Polymers 0.000 claims description 15
- 239000004645 polyester resin Substances 0.000 claims description 15
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- 239000011258 core-shell material Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 10
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 9
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- 235000000126 Styrax benzoin Nutrition 0.000 claims description 8
- 235000008411 Sumatra benzointree Nutrition 0.000 claims description 8
- 229960002130 benzoin Drugs 0.000 claims description 8
- 235000019382 gum benzoic Nutrition 0.000 claims description 8
- 239000000155 melt Substances 0.000 claims description 8
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- 238000007872 degassing Methods 0.000 claims description 6
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- 239000000049 pigment Substances 0.000 claims description 6
- 150000003512 tertiary amines Chemical class 0.000 claims description 6
- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 claims description 5
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- 239000000463 material Substances 0.000 claims description 4
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- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 2
- FUIQBJHUESBZNU-UHFFFAOYSA-N 2-[(dimethylazaniumyl)methyl]phenolate Chemical compound CN(C)CC1=CC=CC=C1O FUIQBJHUESBZNU-UHFFFAOYSA-N 0.000 claims description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 150000008064 anhydrides Chemical class 0.000 claims description 2
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 claims description 2
- 150000002825 nitriles Chemical class 0.000 claims description 2
- 229920003986 novolac Polymers 0.000 claims description 2
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 2
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 24
- 238000012360 testing method Methods 0.000 description 18
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 5
- LFMQNMXVVXHZCC-UHFFFAOYSA-N 1,3-benzothiazol-2-yl n,n-diethylcarbamodithioate Chemical compound C1=CC=C2SC(SC(=S)N(CC)CC)=NC2=C1 LFMQNMXVVXHZCC-UHFFFAOYSA-N 0.000 description 4
- FUOZJYASZOSONT-UHFFFAOYSA-N 2-propan-2-yl-1h-imidazole Chemical compound CC(C)C1=NC=CN1 FUOZJYASZOSONT-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- QAEKNCDIHIGLFI-UHFFFAOYSA-L cobalt(2+);2-ethylhexanoate Chemical compound [Co+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O QAEKNCDIHIGLFI-UHFFFAOYSA-L 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
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- 238000011416 infrared curing Methods 0.000 description 4
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- BKCCAYLNRIRKDJ-UHFFFAOYSA-N 2-phenyl-4,5-dihydro-1h-imidazole Chemical compound N1CCN=C1C1=CC=CC=C1 BKCCAYLNRIRKDJ-UHFFFAOYSA-N 0.000 description 1
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- Paints Or Removers (AREA)
Abstract
The invention relates to a powder coating, a preparation method and application thereof, wherein the powder coating comprises the following components in parts by weight: 50-100 parts of matrix resin, 2-25 parts of curing agent, 0.5-8 parts of composite curing accelerator and 0.1-5 parts of nano filler; the composite curing accelerator comprises nano rubber particles and a liquid tertiary amine catalyst loaded on the nano rubber particles. The powder coating provided by the invention applies the more efficient liquid tertiary amine catalyst to a solid powder coating system, so that the selection range of the curing accelerator for the powder coating is expanded; and the powder coating has the advantages of short curing time and low curing temperature, and the coating formed after curing has good impact strength, adhesive force, solvent resistance, acid resistance, alkali resistance, moist heat resistance and neutral salt fog resistance, and is suitable for coating heat-sensitive substrates such as wood, engineering plastics, glass, paper and the like.
Description
Technical Field
The invention belongs to the technical field of coating compositions, and particularly relates to a powder coating and a preparation method and application thereof.
Background
The powder coating is solid powder environment-friendly coating without any organic solvent, but the powder coating has the problem of higher curing temperature, so that the low-temperature curing powder coating becomes a research hot spot in the coating industry in recent years, but the coating formed after the powder coating is cured under the low-temperature curing condition has the problem that the physical and chemical properties such as impact strength, bending strength, adhesive force and the like cannot meet the performance requirements, and further application of the powder coating is hindered. Therefore, it is of great importance to prepare powder coatings having a low curing temperature and excellent overall properties.
When the low-temperature curing powder coating is prepared in the prior art, a mode of adding high-activity resin or curing accelerator is mainly adopted. CN116041676a discloses a polyester resin for low-temperature curing powder coating and a preparation method thereof, CN115109259a discloses a polyester resin capable of low-temperature curing and a preparation method thereof, but the high-activity low-temperature curing resin is a multi-functional group system, and the coating has poor physical and chemical properties such as flexibility after low-temperature curing. CN106398482a discloses a low-temperature curing powder coating prepared by taking 2-phenylimidazoline as a curing accelerator, in order to adapt to the processing mode of the low-temperature curing powder coating, the invention adopts a solid accelerator, and the curing accelerator has more additive amount and lower catalytic efficiency.
The existing low-temperature curing powder coating is low in catalysis efficiency of a curing accelerator in the powder coating, and poor in physical and chemical properties such as impact strength and adhesive force of a coating after the low-temperature curing powder coating is cured, so that the powder coating which is short in curing time, low in curing temperature and good in physical and chemical properties such as impact strength and adhesive force of the coating after the low-temperature curing is to be developed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a powder coating, a preparation method and application thereof, and the powder coating has lower curing temperature, shorter curing time and excellent physical and chemical properties such as impact strength, adhesive force and the like through the selection and the dosage regulation of each component of the powder coating.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a powder coating, which comprises the following components in parts by weight: 50-100 parts of matrix resin, 2-25 parts of curing agent, 0.5-8 parts of composite curing accelerator and 0.1-5 parts of nano filler; the composite curing accelerator comprises nano rubber particles and a liquid tertiary amine catalyst loaded on the nano rubber particles.
The powder coating provided by the invention can fully absorb medium-wave infrared, and the composite curing accelerator in the powder coating can promote the curing of the powder coating, reduce the curing temperature of the powder coating, shorten the curing time and improve the flexibility and adhesive force of a coating formed after the powder coating is cured; the nano filler can improve the adhesive force of a coating formed after the powder coating is cured, and can regulate the rheological property of the powder coating. According to the invention, the liquid tertiary amine catalyst in the composite curing accelerator is adsorbed on the nano rubber particles, so that the more efficient liquid tertiary amine catalyst can be applied to a solid powder coating system, and the composite curing accelerator is matched with other components of the powder coating in a specific proportion, so that a coating formed after the powder coating is cured has good impact strength, adhesive force, solvent resistance, acid resistance, alkali resistance, moist heat resistance and neutral salt fog resistance.
The matrix resin may be 50 to 100 parts by weight, for example, 50 parts by weight, 55 parts by weight, 60 parts by weight, 65 parts by weight, 70 parts by weight, 75 parts by weight, 80 parts by weight, 85 parts by weight, 90 parts by weight, 95 parts by weight or 100 parts by weight, and specific point values among the above point values are limited in length and for brevity, the present invention is not exhaustive of the specific point values included in the range.
The curing agent is 2-25 parts by weight, for example, 2 parts by weight, 4 parts by weight, 6 parts by weight, 8 parts by weight, 10 parts by weight, 12 parts by weight, 14 parts by weight, 16 parts by weight, 18 parts by weight, 20 parts by weight, 22 parts by weight, 24 parts by weight or 25 parts by weight, and specific point values among the above point values are limited in length and for brevity, and the present invention is not exhaustive of the specific point values included in the range.
The compound curing accelerator is 0.5 to 8 parts by weight, for example, 0.5 part by weight, 1 part by weight, 1.5 parts by weight, 2 parts by weight, 3 parts by weight, 4 parts by weight, 5 parts by weight, 6 parts by weight, 7 parts by weight or 8 parts by weight, and specific point values between the above point values are limited in length and for brevity, the present invention is not exhaustive of the specific point values included in the range.
The nanofiller may be present in an amount of 0.1 to 5 parts by weight, for example, 0.1 part by weight, 0.5 part by weight, 1 part by weight, 1.5 parts by weight, 2 parts by weight, 2.5 parts by weight, 3 parts by weight, 3.5 parts by weight, 4 parts by weight, 4.5 parts by weight or 5 parts by weight, and specific point values between the above point values, and the present invention is not intended to be exhaustive of the specific point values included in the range for brevity and conciseness.
The following is a preferred technical scheme of the present invention, but not a limitation of the technical scheme provided by the present invention, and the following preferred technical scheme can better achieve and achieve the objects and advantages of the present invention.
As a preferred embodiment, the matrix resin includes a combination of a first resin and a second resin.
Preferably, the mass of the second resin is less than or equal to 50% based on 100% of the mass of the matrix resin, and may be, for example, 0, 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45% or 50%, and specific point values between the above point values, which are limited in space and for the sake of brevity, the present invention is not exhaustive.
Preferably, the first resin comprises a combination of a low viscosity epoxy resin and a high viscosity epoxy resin.
The high-viscosity epoxy resin is favorable for dispersing the nano rubber particles, can improve the physical and chemical properties of a coating formed after the powder coating is cured, and can promote the dispersion of the liquid tertiary amine catalyst by good dispersion of the nano rubber particles; the low-viscosity epoxy resin has more reactive functional groups, so that the activity of the powder coating can be improved, and the curing of the powder coating can be promoted.
Preferably, the low viscosity epoxy resin has a mass of 10-30%, such as 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, 26%, 28% or 30%, based on 100% of the mass of the first resin, and specific point values between the above point values are limited in space and for brevity, the present invention is not exhaustive of the specific point values included in the range.
Preferably, the low viscosity epoxy resin includes any one or a combination of at least two of a first bisphenol a type epoxy resin, a bisphenol F type epoxy resin, or a novolac epoxy resin.
Preferably, the high viscosity epoxy resin comprises a second bisphenol a type epoxy resin.
Preferably, the melt viscosity of the first bisphenol a type epoxy resin and the novolac epoxy resin at 150 ℃ is each independently 300 to 4000mpa.s, for example, 300mpa.s, 500mpa.s, 800mpa.s, 1000mpa.s, 1300mpa.s, 1500mpa.s, 2000mpa.s, 2200mpa.s, 260 mpa.s, 2800mpa.s, 3000mpa.s, 3200mpa.s, 3400mpa.s, 3600mpa.s, 3800mpa.s or 4000mpa.s, and specific point values between the above point values are limited to a spread and for brevity, the present invention does not exhaustively list the specific point values included in the range.
Preferably, the high viscosity epoxy resin has a melt viscosity of 6000 to 13000mpa.s at 150 ℃, for example, 6000mpa.s, 7000mpa.s, 780 mpa.s, 9000mpa.s, 10000mpa.s, 11000mpa.s, 12000mpa.s or 13000mpa.s, and specific point values between the above point values, which are limited in space and for brevity, the present invention is not exhaustive.
Preferably, the second resin includes any one or a combination of at least two of a carboxyl polyester resin, a hydroxyl polyester resin, or a carboxyl acrylic resin.
In the powder coating provided by the invention, the second resin has higher functional group content, and can play roles in promoting the curing of the powder coating and improving the crosslinking density.
Preferably, the carboxylic polyester resin has an acid value of 50 to 70mg KOH/g, for example, 50mg KOH/g, 52mg KOH/g, 54mg KOH/g, 56mg KOH/g, 58mg KOH/g, 60mg KOH/g, 62mg KOH/g, 64mg KOH/g, 66mg KOH/g, 68mg KOH/g or 70mg KOH/g, and specific point values between the above point values, are limited in length and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the range.
Preferably, the hydroxyl value of the hydroxyl polyester resin is 100 to 220mg KOH/g, and may be, for example, 100mg KOH/g, 110mg KOH/g, 120mg KOH/g, 130mg KOH/g, 140mg KOH/g, 150mg KOH/g, 160mg KOH/g, 170mg KOH/g, 180mg KOH/g, 190mg KOH/g, 200mg KOH/g, 210mg KOH/g or 220mg KOH/g, and specific point values between the above point values, are limited in length and for brevity, the invention is not exhaustive of the specific point values included in the range.
Preferably, the carboxylic acrylic resin has an acid value of 140-200mg KOH/g, which may be, for example, 140mg KOH/g, 150mg KOH/g, 160mg KOH/g, 170mg KOH/g, 180mg KOH/g, 190mg KOH/g or 200mg KOH/g, and specific point values between the above point values, are limited in length and for the sake of brevity, the invention is not exhaustive of the specific point values included in the range.
Preferably, the curing agent comprises any one or a combination of at least two of triglycidyl isocyanurate, substituted dicyandiamide, blocked polyisocyanate, dodecanedioic acid, dicarboxylic dihydrazide, anhydride, novolac resin, phenolic hydroxyl resin or hydroxyalkylamide.
Preferably, the nano rubber particles comprise any one or a combination of at least two of nano-nitrile powder rubber particles, nano-carboxyl nitrile powder rubber particles, nano-butylbenzene pyridine powder rubber particles or core-shell nano-rubber particles, and further preferably nano-nitrile powder rubber particles.
Preferably, the core-shell type nano-rubber particles comprise butadiene core-shell type rubber particles and/or acrylic core-shell type rubber particles. In the present invention, the core-shell type nano-rubber particles are all commercially available products, and illustratively, butadiene core-shell type rubber particles are commercially available from kanenaMZ120 of brillouin chemistry.
Preferably, the particle size of the nano-rubber particles is 50-500nm, for example, 50nm, 60nm, 70nm, 80nm, 100nm, 120nm, 140nm, 160nm, 180nm, 200nm, 250nm, 300nm, 350nm, 400nm, 450nm or 500nm, and specific point values between the above point values, are limited in length and for brevity, the present invention is not exhaustive of the specific point values included in the range.
Preferably, the liquid tertiary amine catalyst comprises any one or a combination of at least two of linear alkyl tertiary amine, triethanolamine, triethylenediamine, dimethylaminomethyl phenol or tris (dimethylaminomethyl) phenol.
Preferably, the straight-chain alkyl-containing tertiary amine comprises any one or a combination of at least two of dodecyl dimethyl tertiary amine, hexadecyl dimethyl tertiary amine, tetradecyl dimethyl tertiary amine or octadecyl dimethyl tertiary amine.
Preferably, the mass ratio of the nano rubber particles to the liquid tertiary amine catalyst is (4-15): 1, for example, may be 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, 10:1, 11:1, 12:1, 13:1, 14:1, 15:1, or the like.
Preferably, the nanofiller comprises any one or a combination of at least two of nano-boehmite, nano-cellulose or nano-silica.
Preferably, the composite curing accelerator is prepared by a method comprising the following steps: mixing the nano rubber particles with the liquid tertiary amine catalyst, and adsorbing the liquid tertiary amine catalyst on the nano rubber particles to obtain the composite curing accelerator.
Preferably, the mixing is for a period of time of 20-60s, for example, 20s, 22s, 24s, 26s, 28s, 30s, 32s, 34s, 36s, 38s, 40s, 44s, 48s, 50s, 52s, 54s, 56s, 58s or 60s, and specific point values between the above point values, are limited in space and for brevity, the invention is not exhaustive of the specific point values included in the range.
Preferably, the temperature of the mixture is 20-35 ℃, such as 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃, 30 ℃, 32 ℃, 34 ℃ or 35 ℃, and specific point values between the above point values, are limited in space and for the sake of brevity, the invention is not exhaustive of the specific point values comprised in the range.
Preferably, the powder coating further comprises 0.1 to 0.5 parts by weight of a degassing agent, for example, 0.1, 0.2, 0.3, 0.4 or 0.5 parts by weight, and specific point values between the above point values, which are limited in space and for brevity, the invention is not intended to be exhaustive.
Preferably, the degassing agent comprises benzoin.
Preferably, the powder coating further includes 0.2 to 1 part by weight of a leveling agent, for example, 0.2 part by weight, 0.3 part by weight, 0.4 part by weight, 0.5 part by weight, 0.6 part by weight, 0.7 part by weight, 0.8 part by weight, 0.1 part by weight or 0.8 part by weight, and specific point values between the above point values, are limited in length and for brevity, the present invention is not exhaustive of the specific point values included in the range.
Preferably, the leveling agent comprises any one or a combination of at least two of acrylate polymer leveling agents.
Preferably, the powder coating further comprises 0.1 to 0.5 parts by weight of pigment, for example, 0.1 part by weight, 0.2 part by weight, 0.3 part by weight, 0.4 part by weight or 0.5 part by weight, and specific point values between the above point values, are limited in space and for brevity, the present invention is not exhaustive of the specific point values included in the range.
Preferably, the pigment comprises any one or a combination of at least two of rutile titanium dioxide, iron oxide yellow, phthalocyanine blue, phthalocyanine green, iron oxide red or ultramarine blue.
Preferably, the curing temperature of the powder coating is 125-135 ℃.
Preferably, the method of curing the powder coating comprises infrared curing.
Preferably, the infrared curing power is 5-20kW/m 2 For example, may be 5kW/m 2 、8kW/m 2 、10kW/m 2 、12kW/m 2 、14kW/m 2 、16kW/m 2 、18kW/m 2 Or 20kW/m 2 And the particular values between the above-mentioned values, are limited in space and for brevity, the invention is not intended to exhaustively enumerate the specific values included in the range.
Preferably, the time of the infrared curing is 3-8min, for example, 3min, 4min, 5min, 6min, 7min or 8min, and the specific point values among the above point values are limited in space and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the range.
In a second aspect, the present invention provides a process for preparing a powder coating as described in the first aspect, the process comprising: and mixing the matrix resin, the curing agent, the composite curing accelerator and the nano filler, and then carrying out melt extrusion, tabletting, cooling, crushing and screening in sequence to obtain the powder coating.
Preferably, the mixed material further comprises a degassing agent, a leveling agent and a pigment.
Preferably, the melt extrusion temperature is 80-110 ℃, such as 80 ℃, 85 ℃, 88 ℃,90 ℃, 95 ℃, 98 ℃, 100 ℃, 102 ℃, 105 ℃, 108 ℃, or 110 ℃, and specific values between the above, are limited in space and for simplicity, the invention is not exhaustive of the specific values included in the range.
Preferably, the particle size is 10 to 100 μm (e.g., 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 100 μm, etc.), more preferably 20 to 80 μm (e.g., 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm or 80 μm, etc.) by the pulverization.
Preferably, the mesh number of the sieving screen is 140-200 mesh, for example, 140 mesh, 170 mesh, 180 mesh or 200 mesh.
In a third aspect, the present invention provides a powder coating as described in the first aspect for use in the coating of a heat-sensitive substrate.
Compared with the prior art, the invention has the following beneficial effects:
(1) The powder coating provided by the invention can be used for applying the liquid tertiary amine catalyst of the traditional epoxy resin to the solid powder coating, so that the dispersion of the liquid tertiary amine catalyst is promoted, the catalytic efficiency of the liquid tertiary amine catalyst is improved, and the selection range of the curing accelerator for the powder coating is expanded;
(2) The powder coating provided by the invention has the advantages of low curing temperature, short curing time, high surface evenness of the coating after low-temperature curing, no pinhole shrinkage cavity, high impact strength of the coating formed after curing at 125-135 ℃, 100-120cm impact performance, 0 level adhesive force, no light-loss softening phenomenon after 100 times of solvent resistance test, no foaming and falling phenomenon after 240 hours of acid resistance test, no foaming and falling phenomenon after 240 hours of alkali resistance test, no light-loss foaming phenomenon after 1000 hours of wet heat resistance test, and no rust point foaming phenomenon after 1000 hours of neutral salt fog resistance test.
Detailed Description
To facilitate understanding of the present invention, examples are set forth below. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Some of the component sources in the examples and comparative examples are as follows:
(1) Low viscosity epoxy resin:
a. bisphenol a epoxy resin: HY902, available from Anhui Hengyuan, has a melt viscosity of 2000mPa.s at 150 ℃;
KD-211E, commercially available from Guotou chemical industry, has a melt viscosity of 300mPa.s at 150 ℃;
b. novolac epoxy resin: KD-211D and KD-211H obtained from Guotou chemical industry have melt viscosities of 2000mPa.s and 4000mPa.s, respectively;
(2) High viscosity bisphenol a epoxy resin: NPES-904H, NPES-904F and NPES-904HP, available from south Asia, have melt viscosities of 6000mPa.s, 9000mPa.s, 13000mPa.s, respectively;
(3) Carboxyl polyester resin: purchased from Zhan Xin resin 1545, acid value 70mg KOH/g;
(4) Carboxyl acrylic resin: purchased from G152, acid number 155mg KOH/G;
(5) Hydroxyl polyester resin: purchased from P1413, hydroxyl number was 100mg KOH/g;
(6) Nano-sized nitrile powder rubber particles: VP401 from Yanshan petrochemical industry, particle size 80-120nm;
(7) Nano carboxyl nitrile powder rubber particles: VP501, available from Yanshan petrochemical industry, has a particle size of 80-120nm;
(8) Butadiene core-shell rubber particles: kanena MZ120, available from brillouin chemistry, particle size 100-200nm;
(9) Nano boehmite: purchased from Xuancheng Jingrui New Material Co., ltd, particle size of 10-15nm;
(10) Nano silicon oxide: purchased from the city of Xuancheng Jinrui New Material Co., ltd, D50 was 30nm;
(11) Leveling agent: GLP588 available from Ningbo south sea chemical Co., ltd;
(12) Substituted dicyandiamides: XB2632 from Ciba;
(13) Blocked polyisocyanates: degussa EP-BF 1320.
Preparation example 1
A composite curing accelerator A, which comprises nanometer butyronitrile powder rubber particles VP401 and hexadecyldimethyl tertiary amine loaded thereon, the preparation method of the composite curing accelerator A comprises the following steps: and (3) mixing 7.5 parts by weight of nano-nitrile powder rubber particles VP401 and 0.5 part by weight of hexadecyl dimethyl tertiary amine at a high speed at 24000r/min by a high-speed mixer for 30 seconds, and adsorbing the hexadecyl dimethyl tertiary amine on the nano-nitrile powder rubber particles VP401 to obtain the composite curing accelerator A.
Preparation example 2
A composite curing accelerator B comprises nano carboxyl nitrile powder rubber particles VP501 and octadecyl dimethyl tertiary amine loaded on the nano carboxyl nitrile powder rubber particles VP501, and the preparation method of the composite curing accelerator B comprises the following steps: 4 parts by weight of nano carboxyl nitrile powder rubber particles VP501 and 1 part by weight of octadecyl dimethyl tertiary amine are mixed at high speed for 30s by a high-speed mixer at the rotating speed of 24000r/min, and then the octadecyl dimethyl tertiary amine is adsorbed on the nano carboxyl nitrile powder rubber particles VP501, so that the composite curing accelerator B is obtained.
Preparation example 3
A composite curing accelerator C comprises nano carboxyl nitrile powder rubber particles VP501 and tetradecyl dimethyl tertiary amine loaded on the nano carboxyl nitrile powder rubber particles VP501, and the preparation method of the composite curing accelerator C comprises the following steps: and (3) mixing 12 parts by weight of nano carboxyl nitrile powder rubber particles VP501 and 1 part by weight of tetradecyl dimethyl tertiary amine at a high speed of 24000r/min by a high-speed mixer for 30s, and adsorbing the tetradecyl dimethyl tertiary amine on the nano carboxyl nitrile powder rubber particles VP501 to obtain the composite curing accelerator C.
Preparation example 4
The preparation method of the composite curing accelerator D comprises the steps of: and (3) mixing 10 parts by weight of nano carboxyl nitrile powder rubber particles VP501 and 1 part by weight of triethanolamine at a high speed at a rotating speed of 24000r/min for 30 seconds by a high-speed mixer, and adsorbing the triethanolamine on the nano carboxyl nitrile powder rubber particles VP501 to obtain the composite curing accelerator D.
Preparation example 5
A composite curing accelerator E comprising butadiene core-shell rubber particles and hexadecyldimethyl tertiary amine supported thereon, the preparation method of the composite curing accelerator E comprising: and (3) mixing 9 parts by weight of butadiene core-shell rubber particles and 1 part by weight of hexadecyl dimethyl tertiary amine at a high speed at 24000r/min by a high-speed mixer for 30 seconds, and adsorbing the hexadecyl dimethyl tertiary amine on the butadiene core-shell rubber particles to obtain the composite curing accelerator E.
Preparation example 6
A composite curing accelerator F comprising nano-nitrile powder rubber particles VP401 and hexadecyldimethyl tertiary amine supported thereon, the preparation method of the composite curing accelerator F comprising: 3 parts by weight of nano-nitrile powder rubber particles VP401 and 1 part by weight of hexadecyl dimethyl tertiary amine are mixed at a high speed for 30 seconds by a high-speed mixer at the rotating speed of 24000r/min, and then the hexadecyl dimethyl tertiary amine is adsorbed on the nano-nitrile powder rubber particles VP401, so that the composite curing accelerator F is obtained.
Preparation of comparative example 1
A composite curing accelerator G comprises nano carboxyl nitrile powder rubber particles VP501 and 2-isopropyl imidazole loaded on the nano carboxyl nitrile powder rubber particles VP501, and the preparation method of the composite curing accelerator G comprises the following steps: and (3) mixing 12 parts by weight of nano carboxyl nitrile powder rubber particles VP501 and 1 part by weight of 2-isopropyl imidazole at a high speed at a rotating speed of 24000r/min for 30 seconds by a high-speed mixer, and adsorbing the 2-isopropyl imidazole on the nano carboxyl nitrile powder rubber particles VP501 to obtain the composite curing accelerator G.
Preparation of comparative example 2
A composite curing accelerator H, the preparation method of the composite curing accelerator H comprising: and (3) mixing 12 parts by weight of nano titanium dioxide and 1 part by weight of tetradecyldimethyl tertiary amine at a high speed for 30 seconds by a high-speed mixer at a rotating speed of 24000r/min to obtain the composite curing accelerator H.
Example 1
The powder coating comprises the following components in parts by weight: bisphenol A type epoxy resin NPES-906 HP 35 weight portions, bisphenol A type epoxy resin HY90215 weight portions, substituted dicyandiamide 2 weight portions, composite curing accelerator A8 weight portions, nano boehmite 0.1 weight portions, benzoin 0.1 weight portions, leveling agent GLP5880.2 weight portions and iron oxide yellow 0.1 weight portions.
The preparation method of the powder coating comprises the following steps: mixing the above components, carrying out twin-screw melt extrusion at 90 ℃ and then tabletting, cooling and crushing to a particle size of 10-100 mu m, and sieving with a 180-mesh sieve to obtain the powder coating.
Example 2
The powder coating comprises the following components in parts by weight: bisphenol A type epoxy resin NPES-906 HP 35 weight portions, bisphenol A type epoxy resin HY90215 weight portions, carboxyl polyester resin 30 weight portions, triglycidyl isocyanurate 3 weight portions, composite curing accelerator B0.5 weight portions, nano boehmite 1 weight portions, benzoin 0.2 weight portions, leveling agent GLP5880.5 weight portions and iron oxide yellow 0.2 weight portions.
The powder coating preparation method differs from example 1 only in that the powder coating components are those provided in this example, and other process parameters and steps are the same as in example 1.
Example 3
The powder coating comprises the following components in parts by weight: 40 parts of bisphenol A type epoxy resin NPES-906F, 90 parts of bisphenol A type epoxy resin HY90210, 50 parts of carboxyl acrylic resin, 1 part of substituted dicyandiamide, 2 parts of triglycidyl isocyanurate, 8 parts of composite curing accelerator C, 3 parts of nano boehmite, 0.2 part of benzoin, 5880.5 parts of leveling agent GLP and 0.2 part of iron oxide yellow.
The powder coating preparation method differs from example 1 only in that the powder coating components are those provided in this example, and other process parameters and steps are the same as in example 1.
Example 4
The powder coating comprises the following components in parts by weight: 45 parts of bisphenol A type epoxy resin NPES-906F, 5 parts of novolac epoxy resin KD-211D, 40 parts of hydroxyl polyester resin, 13 parts of phenolic hydroxyl resin, 12 parts of closed polyisocyanate, 6 parts of composite curing accelerator D, 5 parts of nano silicon oxide, 0.5 part of benzoin, 5881 parts of leveling agent GLP and 0.5 part of iron oxide yellow.
The powder coating preparation method differs from example 1 only in that the powder coating components are those provided in this example, and other process parameters and steps are the same as in example 1.
Example 5
The powder coating comprises the following components in parts by weight: 40 parts of bisphenol A type epoxy resin NPES-906H, 10 parts of novolac epoxy resin KD-211H, 40 parts of hydroxyl polyester resin, 1.5 parts of substituted dicyandiamide, 12 parts of closed polyisocyanate, 5 parts of composite curing accelerator E, 3 parts of nano silicon oxide, 0.3 part of benzoin, 5880.5 parts of leveling agent GLP and 0.3 part of iron oxide yellow.
The powder coating preparation method differs from example 1 only in that the powder coating components are those provided in this example, and other process parameters and steps are the same as in example 1.
Example 6
A powder coating and a method for preparing the same are different from example 3 only in that the composite curing accelerator C in this example is 12 parts by weight, and other raw materials, process parameters and steps are the same as those in example 3.
Example 7
A powder coating and a method for preparing the same are different from example 3 only in that the bisphenol A type epoxy tree NPES-904F is 50 parts by weight and the bisphenol A type epoxy tree HY902 is not added in the present example, and other raw materials, process parameters and steps are the same as those of example 3.
Example 8
A powder coating and a preparation method thereof are different from example 3 only in that the composite curing accelerator C is replaced by the composite curing accelerator F in equal quantity, and other raw materials, process parameters and steps are the same as those of example 3.
Comparative example 1
A powder coating and a preparation method thereof are different from example 2 only in that the composite curing accelerator B is replaced by the composite curing accelerator G in equal quantity, and other raw materials, process parameters and steps are the same as those of example 2.
Comparative example 2
A powder coating and a preparation method thereof are different from example 3 only in that the composite curing accelerator C is replaced by the composite curing accelerator H in equal quantity, and other raw materials, process parameters and steps are the same as those of example 3.
Comparative example 3
The powder coating comprises the following components in parts by weight: 40 parts of bisphenol A type epoxy resin NPES-906F, 90 parts of bisphenol A type epoxy resin HY90210 parts of carboxyl acrylic resin, 50 parts of substituted dicyandiamide, 2 parts of triglycidyl isocyanurate, 7.4 parts of nano carboxyl nitrile powder rubber particles VP501, 0.6 part of tetradecyl dimethyl tertiary amine, 3 parts of nano boehmite, 0.2 part of benzoin, 5880.5 parts of leveling agent GLP and 0.2 part of iron oxide yellow.
The preparation method of the powder coating material was different from example 3 only in that the components of the powder coating material were the components provided in this comparative example, and other process parameters and steps were the same as in example 3.
The powder coatings provided in examples 1-8 and comparative examples 1-3 were coated on glass fiber reinforced composite substrates by a high voltage electrostatic method, and were formed by infrared curing at a power of 20kW/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The curing time was 5min, and a coating was obtained, and the properties of the coating were tested according to the following method, and the test results are shown in table 1:
(1) The degree of cure and the cure temperature of the coating were measured using DSC (manufacturer: TAinstruments, model: Q1000) and were performed as follows:
a. coating curing degree test: the total heat released when the uncured powder coating was fully cured was measured by DSC to be ΔH 0 (J/g) and the reaction heat remaining when not fully cured was ΔH R (J/g), coating cure degree a= (Δh) 0 -ΔH R )/ΔH 0 ；
b. Curing temperature: performing non-isothermal heating test on the uncured powder coating by DSC to obtain the curing temperature of the powder coating;
(2) Coating thickness: according to GB/T1764 test;
(3) Adhesion force: according to GB/T9286-2021 test, a cutting knife tool is adopted to cut the surface of the coating to form a grid pattern, and the cut edge of the coating is completely smooth to be 0 level; a small amount of coating falls off at the intersection of the incisions, and the affected intersection cutting area is 1 grade with less than 5 percent; coating is removed at the intersection of the incisions or along the edges of the incisions, and the affected cross-cut area is grade 2 with more than 5% and less than 15%;
(4) Impact properties: according to GB/T1732 test, recording the height of the heavy hammer falling on the test plate, and observing whether the coating has the phenomena of cracking, peeling and the like;
(5) Solvent resistance: according to GB/T23989-2009 test, wiping 100 times by butanone, and observing whether the coating has a light-loss softening phenomenon or not;
(6) Acid resistance: according to GB/T9274-1988 test, 3wt% HCl is adopted for soaking for 240 hours, and whether the coating is foamed and falls off or not is observed;
(7) Alkali resistance: according to GB/T9274-1988 test, 5wt% NaOH is adopted for soaking for 240 hours, and whether the coating has foaming and falling phenomena is observed;
(8) Wet heat resistance: according to GB/T1740-2007 test, treating for 1000 hours at 47 ℃ and 96% relative humidity, and observing whether the coating has a light-loss foaming phenomenon;
(9) Neutral salt fog resistance, according to GB/T1771-2007 test, treating with sodium chloride aqueous solution with mass concentration of 50g/L for 1000h, and observing whether the coating has rust point foaming phenomenon.
TABLE 1
As can be seen from the test data in Table 1, the powder coating provided by the invention has the advantages of high curing speed, low curing temperature, and good impact strength, adhesive force, solvent resistance, acid resistance, alkali resistance, wet heat resistance and neutral salt fog resistance. As is clear from the comparison of the examples 6 and 3, if the amount of the composite curing accelerator is too large, the nano rubber particles are agglomerated, the dispersibility of the nano rubber particles in the powder coating is poor, the dispersibility of the liquid tertiary amine catalyst in the powder coating is poor, the curing temperature of the powder coating is increased, the curing speed is reduced, and the impact strength and the adhesive force of the coating are poor; as is clear from a comparison of example 7 and example 3, the low-viscosity epoxy resin can improve the activity of the powder coating, promote the curing of the powder coating, and the removal of the low-viscosity epoxy resin can cause the curing temperature of the powder coating to rise, the curing degree to be reduced, and the solvent resistance, acid resistance, alkali resistance, wet heat resistance and salt spray resistance of the coating to be deteriorated; as is clear from a comparison of example 8 and example 3, a mass ratio of the nano rubber particles to the liquid tertiary amine catalyst is too small, which results in insufficient adsorption and dispersion of the liquid tertiary amine catalyst by the nano rubber particles, resulting in an increase in the curing temperature of the powder coating, a decrease in the curing speed, and deterioration of the adhesion of the coating.
As is clear from the comparison between the example 2 and the comparative example 1, the liquid tertiary amine catalyst has higher catalytic efficiency compared with the 2-isopropyl imidazole, can effectively shorten the curing time of the powder coating, reduce the curing temperature and lead the coating formed by curing the powder coating to have excellent physicochemical properties.
As can be seen from the comparison between the example 3 and the comparative example 2, the use of the nano rubber particles can adsorb the liquid tertiary amine catalyst on the surface, which does not affect the performance of the nano rubber particles in the powder coating, but after the nano titanium dioxide is replaced, the adsorption performance of the nano titanium dioxide on the liquid tertiary amine catalyst is poor, the liquid tertiary amine catalyst cannot be completely adsorbed and dispersed, so that the nano titanium dioxide and the liquid tertiary amine catalyst are mutually adhered and agglomerated, and the catalytic effect of the nano titanium dioxide and the liquid tertiary amine catalyst cannot be effectively exerted, so that the coating performance is poor, the curing temperature of the powder coating is increased, and the curing speed is reduced.
As is clear from the comparison between example 3 and comparative example 3, the nano rubber particles and the liquid tertiary amine catalyst are directly added and used, and the liquid tertiary amine catalyst cannot be uniformly dispersed in the powder coating, so that the curing temperature of the powder coating is increased, the curing speed is reduced, and the coating performance is deteriorated.
The applicant states that the detailed process equipment and process flows of the present invention are described by the above examples, but the present invention is not limited to, i.e., does not mean that the present invention must be practiced in dependence upon, the above detailed process equipment and process flows. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (10)
1. The powder coating is characterized by comprising the following components in parts by weight: 50-100 parts of matrix resin, 2-25 parts of curing agent, 0.5-8 parts of composite curing accelerator and 0.1-5 parts of nano filler;
the composite curing accelerator comprises nano rubber particles and a liquid tertiary amine catalyst loaded on the nano rubber particles.
2. The powder coating of claim 1, wherein the matrix resin comprises a combination of a first resin and a second resin;
preferably, the mass of the second resin is 50% or less based on 100% of the mass of the matrix resin;
preferably, the first resin comprises a combination of a low viscosity epoxy resin and a high viscosity epoxy resin;
preferably, the mass of the low viscosity epoxy resin is 10 to 30% based on 100% of the mass of the first resin;
preferably, the low viscosity epoxy resin comprises any one or a combination of at least two of a first bisphenol a type epoxy resin, a bisphenol F type epoxy resin, or a novolac epoxy resin;
preferably, the high viscosity epoxy resin comprises a second bisphenol a type epoxy resin;
preferably, the melt viscosity of the first bisphenol a type epoxy resin and the novolac epoxy resin at 150 ℃ is each independently 300 to 4000mpa.s;
preferably, the high viscosity epoxy resin has a melt viscosity of 6000-13000mpa.s at 150 ℃;
preferably, the second resin comprises any one or a combination of at least two of a carboxyl polyester resin, a hydroxyl polyester resin, or a carboxyl acrylic resin;
preferably, the carboxylic polyester resin has an acid value of 50 to 70mg KOH/g;
preferably, the hydroxyl polyester resin has a hydroxyl value of 100 to 220mg KOH/g;
preferably, the carboxylic acrylic resin has an acid value of 140-200mg KOH/g.
3. The powder coating of claim 1 or 2, wherein the curing agent comprises any one or a combination of at least two of triglycidyl isocyanurate, substituted dicyandiamide, blocked polyisocyanate, dodecanedioic acid, dicarboxylic dihydrazide, anhydride, novolac resin, phenolic hydroxyl resin, or hydroxyalkylamide.
4. A powder coating according to any one of claims 1-3, wherein the nano-rubber particles comprise any one or a combination of at least two of nano-nitrile powder rubber particles, nano-carboxylated nitrile powder rubber particles, nano-butylbenzene-pyridine powder rubber particles or core-shell nano-rubber particles, preferably nano-nitrile powder rubber particles;
preferably, the core-shell nano-rubber particles comprise butadiene core-shell rubber particles and/or acrylic core-shell rubber particles;
preferably, the particle size of the nano rubber particles is 50-500nm;
preferably, the liquid tertiary amine catalyst comprises any one or a combination of at least two of linear alkyl tertiary amine, triethanolamine, triethylenediamine, dimethylaminomethyl phenol or tris (dimethylaminomethyl) phenol;
preferably, the straight-chain alkyl-containing tertiary amine comprises any one or a combination of at least two of dodecyl dimethyl tertiary amine, hexadecyl dimethyl tertiary amine, tetradecyl dimethyl tertiary amine or octadecyl dimethyl tertiary amine;
preferably, the mass ratio of the nano rubber particles to the liquid tertiary amine catalyst is (4-15): 1, a step of;
preferably, the nanofiller comprises any one or a combination of at least two of nano-boehmite, nano-cellulose or nano-silica.
5. The powder coating of any one of claims 1-4, wherein the composite cure promoter is prepared by a process comprising: mixing the nano rubber particles with the liquid tertiary amine catalyst, wherein the liquid tertiary amine catalyst is adsorbed on the nano rubber particles to obtain the composite curing accelerator;
preferably, the mixing time is 20-60s;
preferably, the temperature of the mixing is 20-35 ℃.
6. The powder coating according to any one of claims 1 to 5, further comprising 0.1 to 0.5 parts by weight of a degassing agent, 0.2 to 1 part by weight of a leveling agent, and 0.1 to 0.5 parts by weight of a pigment.
7. The powder coating of claim 6, wherein the degassing agent comprises benzoin;
preferably, the leveling agent comprises any one or a combination of at least two of acrylate polymer leveling agents;
preferably, the pigment comprises any one or a combination of at least two of rutile titanium dioxide, iron oxide yellow, phthalocyanine blue, phthalocyanine green, iron oxide red or ultramarine blue.
8. A method of preparing a powder coating as claimed in any one of claims 1 to 7, comprising: and mixing the matrix resin, the curing agent, the composite curing accelerator and the nano filler, and then carrying out melt extrusion, tabletting, cooling, crushing and screening in sequence to obtain the powder coating.
9. The method of claim 8, wherein the mixed material further comprises a degassing agent, a leveling agent, and a pigment;
preferably, the temperature of the melt extrusion is 80-110 ℃;
preferably, the particle size is 10 to 100 μm, more preferably 20 to 80 μm by the pulverization;
preferably, the mesh number of the sieving screen is 140-200 mesh.
10. A powder coating according to any one of claims 1 to 7 for use in the coating of heat-sensitive substrates.
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